7-(2-Chloroethyl)theophylline → HCID 13534156, Verbindung

HRID 464649Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 464649
Cl[CH2:2][CH2:3][N:4]1[C:12]2[C:11](=[O:13])[N:10]([CH3:14])[C:9](=[O:15])[N:8]([CH3:16])[C:7]=2[N:6]=[CH:5]1.[NH:17]1[CH2:22][CH2:21][CH:20]([C:23]2[C:31]3[C:26](=[CH:27][CH:28]=[C:29]([OH:32])[CH:30]=3)[NH:25][CH:24]=2)[CH2:19][CH2:18]1.C(=O)([O-])[O-].[Na+].[Na+].[I-].[K+]>CC(C)CC(=O)C>[OH:32][C:29]1[CH:30]=[C:31]2[C:26](=[CH:27][CH:28]=1)[NH:25][CH:24]=[C:23]2[CH:20]1[CH2:21][CH2:22][N:17]([CH2:2][CH2:3][N:4]2[C:12]3[C:11](=[O:13])[N:10]([CH3:14])[C:9](=[O:15])[N:8]([CH3:16])[C:7]=3[N:6]=[CH:5]2)[CH2:18][CH2:19]1

Komponenten

6

Edukt 4

HCID 18827-(2-Chloroethyl)theophyllineHCID 4875Potassium IodideHCID 10340Sodium CarbonateHCID 122292493-(4-piperidinyl)-1H-indol-5-ol

Produkt 1

HCID 13534156HCID 13534156, VerbindungAusbeute 43 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 7909Methyl Isobutyl KetoneLösungsmittel

Versuchsvorschrift

A mixture of 3.65 parts of 7-(2-chloroethyl)-3,7-dihydro-1,3-dimethyl-1H-purine-2,6-dione, 3 parts of 3-(4-piperidinyl)-1H-indol-5-ol, 4.25 parts of sodium carbonate, 0.1 parts and potassium iodide and 200 parts of 4-methyl-2-pentanone was stirred and refluxed overnight. The whole was filtered while hot and the filtrate was evaporated. The residue was suspended in 45 parts of trichloromethane and 2.4 parts of methanol. The product was filtered off, washed with 16 parts of methanol and dried, yielding 2.5 parts (43%) of 3,7-dihydro-7-[2-[4-(5-hydroxy-1H-indol-3-yl)-1-piperidinyl]ethyl]-1,3-dimethyl-1H-purine-2,6-dione; mp. 232.5° C. (compound 2).

Aufarbeitung

  1. temperaturerefluxed overnight
  2. filtrationThe whole was filtered while hot and the filtrate
  3. customwas evaporated
  4. filtrationThe product was filtered off
  5. washwashed with 16 parts of methanol
  6. customdried

Quellen und Nachweise

ORD-Eintrag
ord-b1feb3073dc8466e92857eab1695ff2f
Quelldatensatz
uspto-grants-1985_10
Patentnummer
US04548939

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